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Gowerl
and I.P. Rhodes A Review of Techniques in the Lassaigne
Reading, Berkshire
England Sodium-Fusion
The sodium-fusion test forms an es- hot solutions is generally faster than for cold solutions.
sential part of most qualitative organic analyses since Methods of Fusion
it represents a rapid method for the detection of the
presence of various elcments in the substance tested. 1) The most common method is to place the organic
The elements usually tested for are nitrogen, sulfur, sample and sodium a t the bottom of an ignition tube
and the halogens-others being tested for usually only and then to bring about reaction by gentle warming
if their presence is suspected from other evidence. (5, 6, 10-1 2 ) .
Since its original use by Lassaigne in 1843 (1, 2) and This technique has the advantage that it allows ob-
subsequent modification by Jacobsen in 1879 (S), in servation of whether the compound has "active-
which sodium replaced potassium as the active reagent, hydrogen" since, if easily replaceable hydrogen is
the test has altered very little, and basically is still in present, direct reaction with sodium occurs in the cold.
use today. The major disadvantage is that with very volatile
However, despite the fact that in essence this is a materials, the organic substance may very easily be
very simple tcst, and quantitative work has proved its lost from the ignition tube before reaction with sodium
sensitivity (4), poor results are often obtained by can occur.
students a t the bench. This fairly general lack of This still remains the most usual technique used.
dexterity in using this test is also aggravated by the 2) A simple modification of (1) in which the sample
fact that most t.exts on practical organic chemistry and sodium are warmed in the ignition tube on a micro
present details of only two, or perhaps three, of the burner only to the extent of allowing the organic ma-
possible techniques of applying this test, it usually being terial to gently reflux within the tube.
true that under different circumstances different When reaction begins the tube is removed from the
techniques yield the best results. Thus, the present burner and the reaction is allowed to subside.
article is intended to collect together the available This method is applicable to volatile materials or
methods with some indication of the most suitable those which are rather inert. However, for volatile
circumstances in which each one may be best applied. materials very great care is required and other more
I t should be noted that although alternative methods certain methods are available.
of detecting elements in organic compounds have been These methods will now be considered.
developed, such as Middleton's test (5-7) and a recent 3) The organic sample and sodium are placed in the
ignit,ion method using oxygen developed by D. C. bottom of an ignition tube and covered by anhydrous
Ayres (a), these will not be dealt with in this article. sodium carbonate to approximately half-fill the tube.
A review article dealing with the history and some uses More sodium is placed on top of the sodium carbonate
of t,he Lassaigne test entitled "A Lost Century, Las- topped by a little more sodium carbonate. The con-
saigne's Test for Nitrogen" was published by Tucker tents of the tube is tamped down and this is heated
in 1943 (9). over a macro-burner beginning at the top of the tube
Fusion of Sodium and Organic Compound and working down. I n this method, thc sodium
I n all the techniques to be described for fusing metal- carbonate tends to hold the sample in contact with the
sodium long enough for reaction to occur. The sodium
lic sodium with an organic compound, it is generally
best to commence with very gentle heating, a point half-way up the tube acts as a "scavenger" talung up
often not sufficiently stressed in the textbooks. After any vapors of unreacted sample that may permeate up
any reaction has begun, the ignition tube should be re- through the layer of sodium carbonate.
moved from the Bunsen flame until the reaction has al-
A variation of this method is to replace the sodium
most ceased, vhen further heat may be applied. The carbonate by glass-wool (10).
4) The organic sample is placed a t the bottom of the
extent of heating should be gradually increased until
tube and a piece of sodium placed about a quarter of the
no further change appears to be taking place in the
ignit,ion tube. The tube should thcn be raised to red- way from the top of the tube. The sodium is then
heated over a micro-burner until i t melts and the head
heat for a few moments to complete reaction and to
volatilize any unreacted organic material. The red- of molten sodium is allowed to roll down the inside wall
hot tube is then plunged into a boiling-tube, beaker, or of the ignition tube onto the sample a t the bottom.
The heat contained in the molten sodium is generally
evaporating basin containing water, care being taken
to shield the mouth of the vessel with a wire gauze. enough to cause reaction but if reaction does not occur,
the method (2) above may be applied to the contents
Boiling of the water-extract is often advised in text-
of the tube.
books but appears unnecessary although the filtering of
5) I n another method, the sample and sodium are
'Present address: 23 Pon Close, Reading, Berkshire, England. arranged in the ignition tube as in (4). The sodium is